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The main goal of this study is the hierarchical synthesis nanostructure CoNi 2 S 4  on the graphenized pencil lead (GPL) and application as solid phase microextraction (SPME) fiber for determination of environmental pollutants. The synthesized nanostructure fiber was investigated by scanning electron microscope, energy dispersive X-ray, X-ray diffraction, Fourier transforms infrared spectroscopy and thermogravimetric analysis. The efficiency of the modified fiber as a new extraction phase for SPME was evaluated by the determination of polyaromatic hydrocarbons (PAHs) from river water samples. The extracted PAHs were monitored by GC-FID. The affecting parameters on the extraction process such as pH, temperature, salinity, stirring speed, and extraction time were investigated. The analytical parameters for determination of PAHs by CoNi 2 S 4 /GPL fiber were studied. Under the optimized conditions, the linearity range of calibration curve was obtained from 0.0001 to 10 µg L −1 . The range of correlation coefficients ( R2 ) and limits of detections were resulted from 0.998 to 0.987 and 0.0001 to 0.003 µg L −1 , respectively. The proposed fiber was successfully used to evaluate PAHs in spiked river samples and RSD % values were obtained in the range of 3.8 − 9.3%.

Modified Graphenized Pencil Lead by CoNi 2 S 4 Nanostructure as a SPME Fiber for Analysis of PAHs from Water Samples